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Nitric Acid → HCID 66745352, 화합물

HRID 1175761
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HRID 1175761 반응식
[O:1]=[C:2]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[O:8][C:4]2([CH2:7][CH2:6][CH2:5]2)[CH2:3]1.OS(O)(=O)=O.[N+:20]([O-])([OH:22])=[O:21]>C(O)(=O)C>[N+:20]([C:12]1[CH:13]=[CH:14][C:9]2[O:8][C:4]3([CH2:7][CH2:6][CH2:5]3)[CH2:3][C:2](=[O:1])[C:10]=2[CH:11]=1)([O-:22])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric Acid2회HCID 58237899spiro[chroman-2,1'-cyclobutan]-4-one

생성물 1

HCID 66745352HCID 66745352, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of 3,4-Dihydro-4-oxo-spiro[2H-1-benzopyran-2,1′-cyclobutane] (Example 3) (10 mmol) in glacial acetic acid (2 ml), conc. H2SO4 (10 mmol) was added at 0° C. and the mixture was stirred for 10 min. A chilled nitrating mixture [prepared from HNO3 (9 mmol) and Conc. H2SO4 (10 mmol)] was then added very slowly and the reaction mixture was allowed to warm up to room temperature and stirred for 5 h. reaction mixture was then quenched with water and the compound was extracted in dichloromethane. Organic layer was separated, dried on anhydrous MgSO4 and concentrated under vacuum. The crude product was then purified by column chromatography to afford the desired compound as a yellow solid.

후처리

  1. additionwas then added very slowly
  2. stirringstirred for 5 h.
  3. customreaction mixture
  4. customwas then quenched with water
  5. extractionthe compound was extracted in dichloromethane
  6. customOrganic layer was separated
  7. dry with materialdried on anhydrous MgSO4
  8. concentrationconcentrated under vacuum
  9. customThe crude product was then purified by column chromatography

출처 및 근거

ORD 기록
ord-8cdd20c896ac430e849544ca62a77598
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07842703B2

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